Volume 75
International Scientific Journal
Issue 2
published monthly by the
October 2015
World Academy of Materials
Pages 53-62
and Manufacturing Engineering
Various forms of platinum deposited on
carbon nanotubes
A.D. Dobrzańska-Danikiewicz a *, W. Wolany a, D. Łukowiec a, D. Cichocki a,
M. Burda b
a
Faculty of Mechanical Engineering, Silesian University of Technology, Konarskiego 18A,
44-100 Gliwice, Poland
b Department of Materials Science & Metallurgy, University of Cambridge UK, 27 Charles
Babbage Rd, CB3 0FS Cambridge, United Kingdom
* Corresponding e-mail address: [email protected]
ABSTRACT
Purpose: The main purpose of the article is to present interesting forms of platinum at a
nanometric scale. There are multiple fabrication methods of nanoparticles, nanowires and other
forms of platinum, and the methods proposed in the article are simple and effective. They employ
carbon nanotubes in the form of a so-called forest, manufactured by CVD methods and nanotubes
dispergated (in a water or ethylene glycol solution) as templates for deposition of Pt nanoforms.
Design/methodology/approach: Scanning Electron Microscopy (SEM) and Transmission
Electron Microscopy (TEM) were applied for showing the structure and morphology of platinum
nanoforms deposited on carbon nanotubes, and Energy Dispersive Spectroscopy (EDS) was used
for confirming the chemical composition of the analysed structures.
Findings: The microscope examinations carried out with scanning electron microscopy have
shown that platinum may crystallise by assuming the form of, notably, nanoparticles, nanowires
and nanocubes. The structure of carbon nanotubes covered with nanoparticles of Pt at a nanoscale
could have been observed by applying high-resolution transmission electron microscopy.
Practical implications: Carbon nanotubes decorated with Pt nanoparticles and platinum at a
nanometric scale are used as, in particular, an active layer of chemical and biochemical sensors.
In addition, excellent catalytic properties of platinum are used in various industrial processes,
including chemical, automotive and petroleum industry.
Originality/value: Chloroplatinic acid H2PtCl6 is an input substance for producing various forms
of platinum. Platinum exhibits unique physiochemical properties at a nanoscale, different than its
properties at a macro scale. It was confirmed that the selected fabrication method of platinum
nanoforms is effective and simple.
Keywords: Nanomaterials; Platinum; Nanoforms; Carbon nanotubes
Reference to this paper should be given in the following way:
A.D. Dobrzańska-Danikiewicz, W. Wolany, D. Łukowiec, D. Cichocki, M. Burda, Various forms of
platinum deposited on carbon nanotubes, Archives of Materials Science and Engineering 75/2
(2015) 53-62.
MATERIALS
© Copyright by International OCSCO World Press. All rights reserved. 2015
53
A.D. Dobrzańska-Danikiewicz, W. Wolany, D. Łukowiec, D. Cichocki, M. Burda
1. Introduction
Introduction
Nanomaterials, also referred to as materials with
a nanometric structure, are characterised by the fact that
their structural elements in at least one direction have
a dimension of not more than 100 nanometres. The
nanostructural layers are referred to as layers deposited
or produced on a given substrate with the predefined
thickness of below 1 µm [1-7]. The following groups of
nanostructured materials (NSMs) can be distinguished
[1,2,6]: (i) zero-dimensional (0D), also called points, e.g.
quantum dots, nanoparticles; (ii) one-dimensional (1D),
e.g. nanowires, nanorods, nanotubes; (iii) two-dimensional (2D), e.g. nanolayers, nanoplates, nanostructured
films; (iv) three-dimension groups (3D) consisting of 0D,
1D and/or 2D objects.
Nanoparticles are usually defined as material particles
dimensioned between 1 and 100 nm and exhibiting
properties differing largely from the properties of the
same bulk material consisting of larger structural
elements [4,8]. Nanoparticles can either have
a crystalline or amorphous structure [5]. The following
materials can be distinguished among other nanomaterials having, similar to nanoparticles, a small aspect
ratio, defined as a ratio of length to diameter:
nanopyramids [9], nanocubes [10,11], nanobeads [12],
nanodiamonds [13]. Research circles are also very
interested in diverse one-dimension nanomaterials (1D).
There is consensus that whiskers and nanorods are
shorter than fibers and nanowires, but definitions of such
nanomaterials have been modified over the last several
years [14-16]. Initially, all one-dimensional nanostructured materials with the diameter varying between
several nanometres to several hundred microns were
referred to as whiskers and nanofibers, while currently
the term fibre rather refers to carbon or polymer
materials [14,17-19]. One-dimensional nanostructured
metallic materials of the similar type with the diameter of
between one atom to several hundred nms are referred to
as nanowires in the current literature [16,20-22], contrary
to nanorods where an aspect ratio, expressed with the
dimension product, is between 3 to 5 [16,20-23]. Onedimension nanostructured materials also encompass
cylindrical carbon nanotubes (CNTs) [24-28] and other
inorganic nanotubes [29,30].
Various nanoparticles fabrication methods exist,
including [7,10,31,32]: (i) vapour condensation
consisting of evaporation of metal in the liquid state and
fast condensation of deposit in the form of clusters with
nanometric dimensions; (ii) grinding, being a disintegration process, and nanoparticles’ sizes are mainly
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54
dependent on the material and grinding time; (iii)
chemical synthesis being the most popular technique
where nanoparticles are formed in a liquid environment
due to reduction reactions of appropriately selected
chemical compounds, e.g. precursors of metals. Nanowires and nanorods are usually manufactured using the
following techniques (Fig. 1) [15,16,20-23,30,33-36]:
(i) chemical synthesis with the chemical growth process
in a gas or liquid environment; (ii) lithography; (iii) selfassembly with templates; (iv) Chemical and Physical
Vapour Deposition; (v) sol-gel method.
Fig. 1. Exemplary methods for fabrication of zero and/or
the one-dimensional nanomaterials
The chemical synthesis method with different
reagents was applied in order to obtain various
nanostructured forms of platinum, including: nanocubes,
nanowires, sea urchins, nanoparticles and nanoaphids,
which are presented in the following chapters of the
article.
Platinum is a ductile metal crystallising in the A1
lattice, with the density of 21.45 g/cm3 and a melting
point of 1772°C and boiling point of 3800°C. Platinum
has widespread practical applications due to its unique
physiochemical properties, very good catalytic
properties, good electrical conductivity. Platinum, also
this occurring at a nanometric scale in diverse forms, is
used in particular in the chemical, petroleum,
automotive, electrical and jewellery sector and in
medicine and dentistry. Chemical and biochemical
substance sensors are an attractive area of such materials’
potential applications, especially Pt nanoparticles
deposited on the surface of carbon nanotubes. It happens
Archives of Materials Science and Engineering
Various forms of platinum deposited on carbon nanotubes
so because it is possible to measure resistance of such
nanomaterials in a time unit in the presence of specific
chemical substances in a liquid and gas environment. The
sensitivity threshold, selectivity and operating speed are
heightened due to deposition of Pt nanoparticles onto the
surface of CNTs as compared to sensors produced with
undeposited CNTs. The nanocomposites consisting of
carbon nanotubes modified with Pt are appropriate for
production of electrodes, they also may be used in
a catalysis process of different chemical reactions and in
fuel cells [33-41].
2. Materials and methodology
2. Materials and methodology
Various forms of platinum in a nanometric form have
been fabricated in the course of research works,
according to the three different variants. Multiwalled
Carbon Nanotubes (MWCNTs) were used each time in
the manufacturing process as a carrier on which
a growth process of various platinum nanoforms took
place. CNTs were employed for the experiments, which
were fabricated in the forest form by Catalytic Chemical
Vapour Deposition (CCVD) with an EasyTube® 2000
device being the equipment of the Department of
Nanotubes and Nanomaterials of the Scientific and
Didactic Laboratory of Nanotechnology and Materials
Technologies at the Institute of Engineering Materials
and Biomaterials, the Silesian University of Technology.
The Authors’ earlier presentations provide thorough
descriptions of the carbon nanotubes forest fabrication
method in the CCVD process together with a description
of the structure of the fabricated MWCNTs [28,42,43].
The carbon nanotubes produced on a silicon substrate
in the form of a forest, i.e. simple cylindrically rolled
graphene layers densely laid next to each other, were
employed twice during the research works undertaken.
A fragment of a nanotubes forest produced on a silicon
plate was used directly in variant 1 for further
experiments, while in variant 2, after separating
nanotubes mechanically from the substrate, they were
functionalised, filtered and dried, and then dispergated
in ethylene glycol. Non-functionalised MWCNTs were
used for implementing variant 3 of the Pt nanoforms
production process, Chemical Vapour Deposition (CVD)
was used at a Cambridge University laboratory [44],
which were dispergated in deionised water in advance.
The detailed conditions of the platinum manufacturing
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Issue 2 October 2015
process in the nanometric form for the three undertaken
variants are presented in Table 1.
Carbon nanotubes in all the variants were used as
templates in the process of manufacturing various
nanoforms of platinum by way of chemical synthesis.
The manufacturing process in variant 1 and 3 was
performed at room temperature in a water solution
without a stabilising agent. H2PtCl6 as a Pt precursor and
formic acid HCOOH as a reducer were used in order to
carry out a chemical reduction process and to produce
platinum atoms which next, in a self-assembly process,
have created its various nanoforms. The chemical
synthesis applied is characterised by an easy and
effective manufacturing process, as a result of which
this method enjoys considerable interest of research
environments globally. For example, by applying carbon
nanotubes doped with nitride (10.4% N) as templates in
the chemical synthesis process, ultra-thin platinum
nanowires with the diameter of about 2.5 nm and length
of up to 100 nm were produced [40]. Another reducer,
i.e. NaBH4, was used in variant 2 [41], which allowed to
fabricate an MWCNT-Pt-type nanocomposite through
deposition - on the surface of carbon nanotubes - of
single platinum nanocrystals with the size of several nm,
with the carbon nanotubes functionalised in prior in
a mixture of HNO3/H2SO4 acids at a rate of 1:3. The
process was assisted mechanically with ultrasounds for
the purpose of functionalisation or using a magnetic
stirrer to ensure appropriate decoration process. The
platinum-decorated nanotubes were filtered and rinsed
with deionised water several times at the final stage.
The Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Scanning
Transmission Electron Microscopy (STEM) techniques
were used to examine the platinum nanoforms achieved
in the experiments. SEM images were made using
a scanning electron microscope SEM Supra 35 by Carl
Zeiss equipped with an X radiation spectrometer of
energy dispersion EDS by EDAX. TEM and STEM
images were taken using a transmission electron
microscope STEM TITAN 80-300 by FEI fitted with an
electron gun with FEG field emission, a condenser
spherical aberration corrector, STEM scanning system,
bright and dark field detectors, HAADF (High Angle
Annular Dark Field), and EFTEM energy image filter
and an EDS spectrometer. The preparations for the
studies for TEM were prepared by collecting materials
from particular samples, placing a droplet of mixtures on
HRTEM nets and drying the preparations at free air at
room temperature.
55
A.D. Dobrzańska-Danikiewicz, W. Wolany, D. Łukowiec, D. Cichocki, M. Burda
Table 1. The conditions of the platinum manufacturing process in the nanometric form for the three undertaken variants
Criterion
VARIANT 1
VARIANT 2
VARIANT 3
MWCNTs
CCVD method at Silesian
CCVD method at Silesian
CVD method at Cambridge
fabrication method
University of Technology
University of Technology
University
Form of MWCNTs
Forest of carbon nanotubes
Carbon nanotubes
Non-functionalised carbon
used in the
functionalised in prior and
nanotubes, dispergated in
experiment
dispergated in glycol ethylene
deionised water
Metal precursor
H2PtCl6
H2PtCl6
H2PtCl6
Reducer
HCOOH
NaBH4
HCOOH
Other substances
H2O
Ethylene glycol, acetone
H2O
Decoration process
72 h
8h
72 h
time
Process temperature Room temperature
140°C
Room temperature
Mechanical
None
Ultrasounds,
Ultrasounds
assistance
magnetic stirrer
Manufacturing
Chemical reduction, selfChemical reduction
Chemical reduction, selfmethod
assembly, spontaneous
assembly, spontaneous growth
growth
Additional activities Washing with deionised
Filtration
Filtration
water of silicon substrate
with Pt deposited on
nanotube forest
Carpet consisting of different Single Pt nanoparticles with
Nanoaphids which are platinum
Manufacturing
process outcome
Pt nanoforms, including:
the size of 3-4 nm arranged
nanoparticles deposited in
uniformly on the surface of
clusters on non-functionalised
nanocubes and nanowires
forming sea urchins
carbon nanotubes
carbon nanotubes
3. Results and
and discussion
discussion
The material manufactured in the technological
conditions characterised in Table 1, as variant 1, was
subject to observations using a scanning electron
microscope. The observations made have permitted to
conclude that the surface formed by a forest of carbon
nanotubes is a place where platinum agglomerates are
attached. It was confirmed in particular that, by way of
self-assembly, a specific platinum carpet was created by
itself on the surface being a forest of MWCNTs,
containing the clusters of platinum creating a less or more
uniform layer (Fig. 2). The topography of the so created
platinum carpet is therefore complex and inhomogeneous.
The microscope observations performed for the
magnification of 20 KX enable to confirm the existence
of oval Pt agglomerates with their size of usually not
more than 1 µm, which is clearly noticeable in
a microscope image in Fig. 3. Observations with even
higher magnification of 100-300 KX allow to state that
the carpet created consists of smaller or larger clusters of
Pt nanocubes and nanowires. The side length of the
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nanocubes (Fig. 4) is less than 100 nm, and nanowires
(Fig. 5) are similar in appearance to thin hairs with the
length of less than 100 nm, which grow in different
directions and create clusters, referred to in the literature
[46,47] as sea urchins, due to the their shape similar to
such underwater animals.
Fig. 2. Platinum precipitates forming a carpet covering
a forest of nanotubes; SEM image
Archives of Materials Science and Engineering
Various forms of platinum deposited on carbon nanotubes
Fig. 3. Oval platinum agglomerates covering a forest of
carbon nanotubes; SEM image
Fig. 4. Pt nanocubes; SEM image
Fig. 5. Pt nanowires forming sea urchins; SEM image
By using the recipe determined in Chapter 2 of the
article, single platinum nanoparticles were deposited onto
the surface of carbon nanotubes as variant 2 of the
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Issue 2 October 2015
manufacturing process. A series of experiments was carried
out in particular using preparations with the 5, 10 and 20%
mass fraction of platinum [41]. MWCNT-5% Pt, MWCNT10% Pt, MWCNT-20% Pt type nanocomposites were
manufactured this way by combining permanently the
carbon-metal material. The experiments made with highresolution electron microscopes have revealed that
a nanocomposite with 5% mass fraction volume of
platinum nanoparticles exhibits the best structure for the
nanocomposites produced during own works [41]. The
material obtained is characterised by highly dispersed Pt
particles on the surface of carbon nanotubes and the lack of
tendency to agglomerate nanoparticles, pointing out that
a deposition process had been performed correctly (Fig. 6).
The uniform arrangement of platinum nanoparticles on the
surface of carbon nanotubes was shown by using an
HAADF detector in the investigations in the STEM mode
and such nanotubes are visible as clear light precipitates
(Fig. 7). It was also ascertained and observed within the
whole volume of the studied nanocomposites that the size
and spherical shape of the fabricated Pt nanoparticles with
the diameter of 3-4 nm was uniform (Fig. 8). Platinum
nanoparticles have a crystalline structure with crystallographic planes clearly visible during STEM observations
using an HAADF detector (Fig. 9).
The images of nanostructured forms of Pt made in
a transmission electron microscope, created according to
the recipe as variant 3 of the manufacturing process
(Table 1), are shown in Figs 10-13. In such case, the selfassembling Pt atoms create nanoforms called nanoaphids
by the authors of the article. The observations made
indicate that platinum nanoparticles exhibit a tendency to
agglomerate in small clusters which are dispersed across
the surface of carbon nanotubes. An HAADF detector was
used during imaging in the STEM mode (Figs 10 and 11)
in order to obtain more exact information about the
arrangement of platinum nanoparticles on the surface of
MWCNTs. Considering the large differences in the value
of atomic numbers of platinum (Z = 78) and carbon
(Z = 6), Pt nanoparticles are visible in the dark field as light
precipitates with an oval, slightly elongated shape, located
in small clusters on the surface of carbon nanotubes.
Changes in the number of Pt nanoparticles on the surface of
nanotubes were noticed in few samples (Fig. 12) while
carrying out observations in the bright field in the STEM
mode, starting with their clear agglomerates (1), through
a high degree of arrangement of small agglomerates (2),
ending with occasional nanoparticle (3). The presence of
platinum nanoparticles as fine agglomerates similar to
aphids in a stalk of a plant are observed in the majority of
cases, which is clearly visible in the dark field (Figs 10-11),
and in the light field (Fig. 13).
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A.D. Dobrzańska-Danikiewicz, W. Wolany, D. Łukowiec, D. Cichocki, M. Burda
58
Fig. 6. Pt nanoparticles deposited on MWCNTs; TEM
image [45]
Fig. 8. Pt nanoparticles deposited on MWCNTs; HRTEM
image [41]
Fig. 7. Pt nanoparticles being light precipitates; STEM
image made with HAADF detector [41]
Fig. 9. Pt nanocrystal with clearly visible crystalline planes,
STEM image made with HAADF detector [41,45]
Qualitative analyses of chemical composition from the
microarea of the carbon-metal preparations were performed
for all three variants of manufacturing process with Energy
Dispersive Spectroscopy (EDS) by EDAX. The elements
forming the given material were each time identified
through an EDS analysis based on a radiation energy
58
Archives of Materials Science and Engineering
Various forms of platinum deposited on carbon nanotubes
value recorded by the instrument expressed with [keV],
which is characteristic for each element. Spectral
qualitative analyses of chemical composition made for
all three variants of manufacturing process show that the
composition of the investigated preparations contain Pt
and C, which is associated to the presence of carbon
nanotubes. Spectroscopic research results made for
variant 2 and variant 3 of the manufacturing process
show the presence of oxygen and cooper. The presence
of Cu is explained by a copper mesh used at the stage of
preparation, onto which the studied materials were
deposited. One from registered EDS spectra made for
variant 2 of nanocomposite manufacturing process is
presented in Fig. 14.
Fig. 10. MWCNTs as stalks covered with Pt nanoaphids;
STEM-HAADF image
Fig. 12. Different number of Pt nanoparticles on carbon
nanotubes; STEM-BF image
Fig. 11. Pt nanoaphids deposited on MWCNTs; STEMHAADF image
Fig. 13. Pt nanoaphids deposited on MWCNTs; STEM-BF
image
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Issue 2 October 2015
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A.D. Dobrzańska-Danikiewicz, W. Wolany, D. Łukowiec, D. Cichocki, M. Burda
fine aphids situated on a stalk of a plant, which, due to their
similarity to the world of nature, have been called
nanoaphids. The experiments undertaken allow to conclude
that, depending on the fabrication method and on the form
of the applied carbon nanotubes, the reducer type and other
chemical compounds used in the manufacturing process,
the time and temperature of the process and the additional
activities performed, nanostructured forms of platinum can
be fabricated with very interesting and diversified morphology.
Acknowledgements
Acknowledgements
Fig. 14. Results of EDS analysis from microarea of
nanomaterial manufactured by variant 2 of the manufacturing process
4. Conclusions
Conclusions
The microscope examinations carried out with scanning
and transmission electron microscopy confirmed that
diverse nanostructured forms of platinum were fabricated,
obtained by carrying out a manufacturing process in line
with three different variants. The authors have developed
diverse nanostructured forms of platinum using a surface of
a forest of multiwalled carbon nanotubes manufactured by
CCVD and walls of functionalised and non-functionalised
MWCNTs as the nucleus places of Pt. Variant 1 of the
manufacturing process has allowed to produce a carpet, on
the surface of a carbon nanotube forest, composed of oval
Pt agglomerates. It can be pointed out by using higher
magnification of 100 KX that such agglomerates include
the clusters of nanocubes and sea urchins made up of
platinum nanowires. The nanowires produced are less than
100 nm long, are homogenous, and the shape of their
agglomerates is similar to carbon nanohorns. By acting
according to variant 2 of the manufacturing process, single
platinum nanoparticles can be deposited onto the surface of
pre-functionalised carbon nanotubes, and the best effect is
achieved for 5% mass fraction of Pt. Single Pt
nanoparticles with the size of 3-4 nm are deposited
uniformly across the entire surface of MWCNTs in such
case. Variant 3 of the manufacturing process enables to
deposit fine Pt agglomerates dispergated in prior in
deionised water onto the surface of non-functionalised
carbon nanotubes, with such agglomerates being similar to
60
60
The works have been implemented within the
framework of the project entitled “Determining the
importance of the effect of the one-dimensional
nanostructural materials on the structure and properties of
newly developed functional nanocomposite and nanoporous materials”, funded by the Polish National Science
Centre in the framework of the “OPUS” competitions. The
project was awarded a subsidy under the decision DEC2012/07/B/ST8/04070.
Additional
Additionalinformation
information
Selected issues related to this paper are planned to be
presented at the 22nd Winter International Scientific
Conference on Achievements in Mechanical and Materials
Engineering Winter-AMME’2015 in the framework of the
Bidisciplinary Occasional Scientific Session BOSS'2015
celebrating the 10th anniversary of the foundation of the
Association of Computational Materials Science and
Surface Engineering and the World Academy of Materials
and Manufacturing Engineering and of the foundation of
the Worldwide Journal of Achievements in Materials and
Manufacturing Engineering.
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